CN111250105A - Clover-type denitration catalyst and preparation method thereof - Google Patents
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0236—Drying, e.g. preparing a suspension, adding a soluble salt and drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/02—Other waste gases
- B01D2258/0283—Flue gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention provides a clover type denitration catalyst and a preparation method thereof, belonging to the technical field of denitration catalysts. The cloverleaf type denitration catalyst provided by the invention comprises a carrier and an active component loaded on the carrier, wherein the carrier is cloverleaf type TiO2‑Al2O3The active components are ferric oxide and manganese dioxide; the mass sum of the ferric oxide and the manganese dioxide accounts for 10-20% of the clover-leaf-type denitration catalyst. The clover-type denitration catalyst has good low-temperature sulfur-resistant denitration performance at the temperature of 180-300 ℃; all in oneThe composite material has higher mechanical property; the catalyst is prepared by using the transition metal oxide, and is non-toxic; the production process is simple and convenient to operate; the catalyst of the invention has small occupied area and convenient loading and unloading.
Description
Technical Field
The invention relates to the technical field of denitration catalysts, and particularly relates to a clover-type denitration catalyst and a preparation method thereof.
Background
At present, current flue gas boiler is various, and the boiler is installed in earlier stage in addition and is made the in-process and do not consider the flue gas denitration, and boiler exhaust gas temperature is on the low side, is less than 300 degrees. The existing denitration technology is mainly a selective reduction denitration reaction, the core of the technology is a denitration catalyst, the service temperature of the existing denitration catalyst is 300-420 ℃, the existing catalyst cannot be used, and the main component of the existing denitration catalyst is V2O5、WO3、TiO2Belonging to hazardous waste, and the replaced catalyst harms the environment. Therefore, the development of a low-temperature, sulfur-resistant, high-activity, non-toxic denitration catalyst is imminent.
Disclosure of Invention
The invention aims to provide a clover type denitration catalyst and a preparation method thereof, and the clover type denitration catalyst is efficient, sulfur-resistant, low in use temperature and easy to industrially apply.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a clover type denitration catalyst, which comprises a carrier and an active component loaded on the carrier, wherein the carrier is clover type TiO2-Al2O3The active components are ferric oxide and manganese dioxide; the mass sum of the ferric oxide and the manganese dioxide accounts for 10-20% of the clover-leaf-type denitration catalyst.
The invention provides a preparation method of the clover type denitration catalyst in the technical scheme, which comprises the following steps:
mixing titanium dioxide, glass fiber, pseudo-boehmite and water to obtain a mixed material;
ageing the mixed material to obtain an aged material;
extruding the stale material to form a clover-shaped material;
subjecting the clover-shaped material to primary calcination to obtain clover-shaped TiO2-Al2O3A carrier;
dissolving an iron source and a manganese source in water to obtain an active solution;
subjecting said clover type TiO to2-Al2O3And (3) soaking the carrier in the active solution, and drying and carrying out secondary calcination in sequence to obtain the clover-type denitration catalyst.
Preferably, the mass ratio of the titanium dioxide, the glass fiber, the pseudo-boehmite and the water is (40-50): 1-4): 15-25): 25-35.
Preferably, the temperature of the ageing is room temperature, and the ageing time is 24 h.
Preferably, the extrusion pressure of the extrusion is 0.2-0.4 Mpa, and the temperature is room temperature.
Preferably, the calcination temperature of the first calcination is 300-500 ℃, and the time is 1-5 h.
Preferably, the molar ratio of the iron element in the iron source, the manganese element in the manganese source and the water is (0.2-0.6): 1: 24.
Preferably, the clover type TiO2-Al2O3The mass solid-liquid ratio of the carrier to the active solution is 1: (0.4 to 1).
Preferably, the drying temperature is 40-80 ℃, and the drying time is 8-16 h.
Preferably, the temperature of the second calcination is 300-500 ℃, and the time is 1-5 h.
The invention provides a clover type denitration catalyst, which comprises a carrier and an active component loaded on the carrier, wherein the carrier is clover type TiO2-Al2O3The active components are ferric oxide and manganese dioxide; the mass sum of the ferric oxide and the manganese dioxide accounts for 10-20% of the clover-leaf-type denitration catalyst. The active components of the clover-type denitration catalyst provided by the invention are ferric oxide and manganese dioxide, wherein a better valence state regulation effect exists between Fe and Mn, so that the clover-type denitration catalyst is preparedThe catalyst has high low-temperature sulfur resistance and good low-temperature sulfur and denitration performance at the temperature of more than 180-300 ℃;
the clover type denitration catalyst provided by the invention is clover type TiO2-Al2O3The catalyst is a carrier, and the carrier has excellent mechanical properties, so that the catalyst also has higher mechanical properties;
the invention provides a preparation method of the clover type denitration catalyst, the catalyst is prepared by using transition metal oxide, and is non-toxic; the production process is simple and convenient to operate; the catalyst of the invention has small occupied area and convenient loading and unloading.
Detailed Description
The invention provides a clover type denitration catalyst, which comprises a carrier and an active component loaded on the carrier, wherein the carrier is clover type TiO2-Al2O3The active components are ferric oxide and manganese dioxide; the mass sum of the ferric oxide and the manganese dioxide accounts for 10-20% of the clover-leaf-type denitration catalyst.
The clover type denitration catalyst provided by the invention comprises a carrier which is clover type TiO2-Al2O3. In the present invention, TiO is contained in the carrier2With Al2O3Is preferably 10: (3-5), more preferably 10: (3.5-4.5).
The clover type denitration catalyst provided by the invention comprises an active component loaded on the carrier, wherein the active component is ferric oxide and manganese dioxide, and the mass ratio of the ferric oxide to the manganese dioxide in the active component is preferably (0.15-0.75): 1, and more preferably (0.3-0.5): 1.
In the invention, the sum of the mass of the ferric oxide and the mass of the manganese dioxide accounts for 10-20% of the weight of the clover-leaf-type denitration catalyst, preferably 12-18%, and more preferably 14.59%.
The invention provides a preparation method of the clover type denitration catalyst in the technical scheme, which comprises the following steps:
mixing titanium dioxide, glass fiber, pseudo-boehmite and water to obtain a mixed material;
ageing the mixed material to obtain an aged material;
extruding the stale material to form a clover-shaped material;
subjecting the clover-shaped material to primary calcination to obtain clover-shaped TiO2-Al2O3A carrier;
dissolving an iron source and a manganese source in water to obtain an active solution;
subjecting said clover type TiO to2-Al2O3And (3) soaking the carrier in the active solution, and drying and carrying out secondary calcination in sequence to obtain the clover-type denitration catalyst.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The invention mixes titanium dioxide, glass fiber, pseudo-boehmite and water to obtain a mixed material. In the invention, the mass ratio of the titanium dioxide, the glass fiber, the pseudo-boehmite and the water is preferably (40-50): 1-4): 15-25): 25-35, more preferably (42-46): 2-3): 16-20): 28-32. In the present invention, the water is preferably deionized water. In the invention, the mixing process is preferably to add water into a stirrer, then add pseudo-boehmite and stir uniformly, then add titanium dioxide and glass fiber and stir uniformly to obtain a mixed material. In the present invention, the rotation speed of the stirring is preferably 30 r/min. In the present invention, titanium dioxide (also known as titanium dioxide TiO)2) The catalyst is not easy to cause chemical change, has better crystal structure, granularity and specific surface area, and is used as a catalyst carrier. In the invention, pseudo-boehmite (alumina monohydrate) is used as a binder, and is compounded with titanium dioxide to be used as a catalyst carrier. The invention utilizes glass fiber to increase the strength of the catalyst.
After the mixed material is obtained, the mixed material is aged to obtain an aged material. In the present invention, the staling is preferably carried out in a conventional staling chamber; the temperature of the ageing is preferably room temperature, and the time of the ageing is preferably 24 h. The invention leads the material to be uniform through aging, improves the plasticity, leads the adhesive (pseudo-boehmite) to better exert the viscosity and is not easy to break when being extruded into three-leaf strips.
After the stale material is obtained, the stale material is extruded to form a clover-shaped material. In the invention, the extrusion pressure of the extrusion is preferably 0.2-0.4 MPa, more preferably 0.25-0.35 MPa, and the temperature is preferably room temperature. The extrusion is preferably carried out in a screw extruder, and the type of the screw extruder is not particularly limited in the invention, and can be selected from types well known in the art. The invention extrudes the material into cloverleaf type by extrusion, thereby leading the contact area of the catalyst to be larger and enhancing the catalytic effect on the basis of reducing the dosage of the catalyst.
After the clover-shaped material is formed, the invention carries out the first calcination on the clover-shaped material to obtain the clover-shaped TiO2-Al2O3And (3) a carrier. Before the first calcination, the clover-shaped material is preferably dried, the drying temperature is preferably 40-80 ℃, more preferably 50-60 ℃, and the drying time is preferably 8-16 hours, more preferably 10-15 hours. The invention removes the moisture in the material by drying. After the drying is finished, the obtained material is subjected to primary calcination, the calcination temperature of the primary calcination is preferably 300-500 ℃, more preferably 350-450 ℃, and the time is preferably 1-5 hours, more preferably 2-3 hours. The strength of the carrier is improved through the first calcination; the clover type TiO2-Al2O3In a support, TiO2And Al2O3Are uniformly dispersed with each other.
The method dissolves an iron source and a manganese source in water to obtain an active solution. In the present invention, the molar ratio of the iron element in the iron source, the manganese element in the manganese source, and water is (0.2-0.6): 1:24, and more preferably (0.3-0.5): 1: 24. In the present invention, the iron source preferably includes iron nitrate or iron acetate, and the manganese source preferably includes manganese acetate or manganese nitrate. The invention takes an iron source and a manganese source as the sources of active components in the catalyst.
After obtaining the active solution, the invention leads the clover type TiO to be2-Al2O3And (3) soaking the carrier in the active solution, and drying and carrying out secondary calcination in sequence to obtain the clover-type denitration catalyst. In the present invention, the clover type TiO2-Al2O3The mass solid-liquid ratio of the carrier to the active solution is preferably 1: (0.4 to 1), more preferably 1: (0.5 to 0.8), and more preferably 1: (0.6-0.7). In the present invention, the time for the immersion is preferably 12 hours, and the temperature is preferably room temperature. The active components in the active solution are loaded on the clover type TiO by dipping2-Al2O3On a carrier.
In the invention, the drying temperature is preferably 40-80 ℃, more preferably 50-60 ℃, and the time is preferably 10-15 h. The invention dries the active solution on the carrier by drying.
In the invention, the second calcination temperature is preferably 300-500 ℃, more preferably 350-450 ℃, and the time is preferably 1-5 hours, more preferably 2-3 hours. According to the invention, the iron source and the manganese source are converted into ferric oxide and manganese dioxide through secondary calcination, and the ferric oxide and the manganese dioxide are used as active components, so that the low-temperature denitration catalyst has excellent low-temperature denitration activity.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 3.2kg of deionized water into a stirrer (the rotating speed is 30r/min), then adding 1.8kg of pseudo-boehmite into the stirrer, uniformly mixing, then adding 5kg of titanium pigment into the stirrer, finally adding 0.2kg of glass fiber, fully mixing the materials to obtain a mixed material, transferring the mixed material to a staling chamber, and carrying out staling at room temperature for 24 hours to obtain a staled substanceFeeding; extruding the stale material at room temperature with a screw extruder under the extrusion pressure of 0.2Mpa to obtain clover type material, drying the clover type material in a drying chamber for 12h (60 deg.C), calcining at 450 deg.C for 3 hr to obtain clover type TiO2-Al2O3A support in which TiO is present2With Al2O3The mass ratio of (A) to (B) is 10: 3;
dissolving ferric nitrate nonahydrate (1.175kg, 2.908mol) and manganese acetate (2.516kg, 14.543mol) in water (6.309kg, 350.5mol) to obtain an active solution, wherein the molar ratio of Fe to Mn is 0.2:1, and mixing the active solution with the clover type TiO2-Al2O3Soaking carrier (10kg) in active solution (10kg) at room temperature for 5 hr, drying the carrier at 60 deg.C for 12 hr, calcining the dried carrier at 450 deg.C for 3 hr to obtain clover type denitration catalyst, denoted as Fe0.2-Mn/TiO2-Al2O3(ii) a In the catalyst, 0.233kg of ferric oxide and 1.265kg of manganese dioxide are contained, the mass ratio of the ferric oxide to the manganese dioxide is 0.184, the total mass of the catalyst is 11.498kg, and the sum of the masses of the ferric oxide and the manganese dioxide accounts for 13 percent of the total mass of the catalyst.
Trifolium type TiO prepared in example 1 was treated by a conventional method2-Al2O3The carrier is subjected to performance test, and is found to have the length of 4-10 mm and the specific surface area of 75m2The mechanical strength is 85N, and the mechanical property of the catalyst cannot be influenced after the active component is loaded, so that the denitration catalyst disclosed by the invention has excellent mechanical property.
Example 2
This example differs from example 1 only in that: ferric nitrate nonahydrate (1.7626kg, 4.362mol) and manganese acetate (2.516kg, 14.543mol), i.e. Fe: Mn (molar ratio) is 0.3:1, and the prepared clover type denitration catalyst is marked as Fe0.3-Mn/TiO2-Al2O3In the catalyst, 0.345kg of ferric oxide, 1.265kg of manganese dioxide, the mass ratio of the ferric oxide to the manganese dioxide is 0.276, the total mass of the catalyst is 11.61kg, and the sum of the masses of the ferric oxide and the manganese dioxide accounts for the catalyst13.9 percent of the total mass of the preparation.
Example 3
This example differs from example 1 only in that: ferric nitrate nonahydrate (2.35kg, 5.816mol) and manganese acetate (2.516kg, 14.543mol), i.e. Fe: Mn (molar ratio) is 0.4:1, and the prepared clover type denitration catalyst is marked as Fe0.4-Mn/TiO2-Al2O3In the catalyst, 0.465kg of ferric oxide and 1.265kg of manganese dioxide are contained, the mass ratio of the ferric oxide to the manganese dioxide is 0.368, the total mass of the catalyst is 11.73kg, and the sum of the mass of the ferric oxide and the mass of the manganese dioxide accounts for 14.7 percent of the total mass of the catalyst.
Example 4
This example differs from example 1 only in that: ferric nitrate nonahydrate (2.94kg, 7.277mol) and manganese acetate (2.516kg, 14.543mol), i.e. Fe: Mn (molar ratio) is 0.5:1, and the prepared clover type denitration catalyst is marked as Fe0.5-Mn/TiO2-Al2O3In the catalyst, 0.582kg of ferric oxide and 1.265kg of manganese dioxide are contained, the mass ratio of the ferric oxide to the manganese dioxide is 0.46, the total mass of the catalyst is 11.847kg, and the sum of the masses of the ferric oxide and the manganese dioxide accounts for 15.6 percent of the total mass of the catalyst.
Example 5
This example differs from example 1 only in that: ferric nitrate nonahydrate (3.525kg, 8.725mol) and manganese acetate (2.516kg, 14.543mol), i.e. Fe: Mn (molar ratio) is 0.6:1, and the prepared clover-type denitration catalyst is marked as Fe0.6-Mn/TiO2-Al2O3In the catalyst, 0.698kg of ferric oxide, 1.265kg of manganese dioxide, 0.5516 mass ratio of the ferric oxide to the manganese dioxide, 11.963kg of total mass of the catalyst and 16.4 percent of the total mass of the ferric oxide and the manganese dioxide are added.
Test example
The clover-type denitration catalyst prepared in the embodiment 1-5 is put into a fixed bed reactor for activity test, and the activity test conditions are as follows: [ NO ]]=[NH3]=400ppm、[O2]=6%,[SO2]50ppm, nitrogen and 8000h of space velocity-1The temperature was 180 ℃ and the specific results are shown in Table 1.
TABLE 1 data of performance test of clover type denitration catalysts prepared in examples 1 to 5
Catalyst and process for preparing same | Inlet NO/ppm | Outlet NO/ppm | Efficiency% |
Fe0.2-Mn/TiO2-Al2O3 | 400 | 150 | 62.5 |
Fe0.3-Mn/TiO2-Al2O3 | 400 | 100 | 75 |
Fe0.4-Mn/TiO2-Al2O3 | 400 | 70 | 82.5 |
Fe0.5-Mn/TiO2-Al2O3 | 400 | 90 | 77.5 |
Fe0.6-Mn/TiO2-Al2O3 | 400 | 95 | 76.25 |
As can be seen from Table 1, the clover-type denitration catalyst prepared by the method has high sulfur-resistant denitration efficiency at a low temperature of 180 ℃.
From the above embodiments, the present invention provides a clover-type denitration catalyst and a preparation method thereof, and the clover-type denitration catalyst has excellent low-temperature sulfur-resistant denitration performance.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A cloverleaf denitration catalyst is characterized by comprising a carrier and an active component loaded on the carrier, wherein the carrier is cloverleaf TiO2-Al2O3The active components are ferric oxide and manganese dioxide; the mass sum of the ferric oxide and the manganese dioxide accounts for 10-20% of the clover-leaf-type denitration catalyst.
2. The method for preparing a clover type denitration catalyst of claim 1, comprising the steps of:
mixing titanium dioxide, glass fiber, pseudo-boehmite and water to obtain a mixed material;
ageing the mixed material to obtain an aged material;
extruding the stale material to form a clover-shaped material;
subjecting the clover-shaped material to primary calcination to obtain clover-shaped TiO2-Al2O3A carrier;
dissolving an iron source and a manganese source in water to obtain an active solution;
subjecting said clover type TiO to2-Al2O3And (3) soaking the carrier in the active solution, and drying and carrying out secondary calcination in sequence to obtain the clover-type denitration catalyst.
3. The preparation method according to claim 2, wherein the mass ratio of the titanium dioxide, the glass fiber, the pseudo-boehmite and the water is (40-50): 1-4): 15-25): 25-35.
4. The preparation method according to claim 2, wherein the temperature of the aging is room temperature, and the time of the aging is 24 hours.
5. The method according to claim 2, wherein the extrusion pressure is 0.2 to 0.4Mpa and the temperature is room temperature.
6. The preparation method according to claim 2, wherein the calcination temperature of the first calcination is 300 to 500 ℃ and the calcination time is 1 to 5 hours.
7. The preparation method according to claim 2, wherein the molar ratio of the iron element in the iron source, the manganese element in the manganese source and the water is (0.2-0.6): 1: 24.
8. The method of claim 2, wherein said clover-type TiO is produced2-Al2O3The mass solid-liquid ratio of the carrier to the active solution is 1: (0.4 to 1).
9. The preparation method according to claim 2, wherein the drying temperature is 40-80 ℃ and the drying time is 8-16 h.
10. The method according to claim 2, wherein the second calcination is carried out at a temperature of 300 to 500 ℃ for 1 to 5 hours.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114160152A (en) * | 2021-12-09 | 2022-03-11 | 山东爱亿普环保科技股份有限公司 | Denitration and decarburization double-effect catalyst and preparation method thereof |
CN114588914A (en) * | 2022-03-21 | 2022-06-07 | 冯垚 | Method for preparing catalyst by using tailings |
WO2023020579A1 (en) * | 2021-08-19 | 2023-02-23 | Basf Corporation | Metal oxide catalyst for selective catalytic reduction |
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2020
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2023020579A1 (en) * | 2021-08-19 | 2023-02-23 | Basf Corporation | Metal oxide catalyst for selective catalytic reduction |
CN114160152A (en) * | 2021-12-09 | 2022-03-11 | 山东爱亿普环保科技股份有限公司 | Denitration and decarburization double-effect catalyst and preparation method thereof |
CN114588914A (en) * | 2022-03-21 | 2022-06-07 | 冯垚 | Method for preparing catalyst by using tailings |
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Application publication date: 20200609 |